Soap and candle and improved process of making the same.



B. E. REUTER.

SOAP AND CANDLE AND IMPROVED PROCESS 0F NIMUNG THE SAME.

APPLICATION FILED APN. 9. 1914A WMe/.web

sin

.To @all whom t may concern.'

known that il, BALTHASAR E. Rnurnn, u. citizen of the United States,residing at Chicago, in the county oi' Cook and State ci illinois, haveinvented a new and iniQ proved Soep enel Candle and improved Irroceee oiMeinne' the Seine, ot which the following is e epeciiicetion.

if have discovered that a soep may be merle 'Within the principle ot'the process of my atent No. 1,068,079, dated July 223 i913, which newarticle of manufacture in that it is a normal harcl soa-p, which, afteron exposure to air end light does not substantially darken or deepen incolor.

nFone, the new Soap oit' my manufacture, icientiecl by the test belowset forth, when removed from its packing box, where air and light arelargely excluded, and placed .upon the dealeris shelf, or put into use,does not turn substantially darker in color, as heretofore, but may evenbecome lighter in color. l

ll have perfected the process of said Pat llo.. 1,068,079 in such manneras to insure obtaining said article of manufacture, enti i -willtherefore proceed 4to repeat the description of the process of saidpatent in euch "aerfected form, and then describe the test unich lieveWorked out for identifying this new article of manufacture.

it has been known that contact with the air increased the discolorationin the Petty acicls7 but no successful means has over been described, sofar as l know, of applying the catalytic saponiiicaiion art to themanutan ture of commercially white or wliitish lin isheti product whichafter an appreciable length of time wouiil not :fiisizolorizc under heinipuence of air and light.

.l have discovered that by (l) iliif'itling the boiiing into sections,enel removing the ribbon or the glycerin liquid (and preti-.r-

both) of the .settling operation7 between Successive boilinge, and (Il)excluding air, il can obtain fatty aciils, the soap from which-Will notl.he .substaniail iliecolorizefl under the conditions existing incooiiiiorcial usage and handling'.

l may employ an appara like that nii-own in lli'o arcompanyinp;'animatie drawing, which may lic described .w follows:

ie the saponiiication tank in section, it :nay be constructed ot" ironwith lenti lin ing, or of wood with icuii in i', or ot' anyacid-resisting material. .lt convergen to the Speoilcetion. of :LettersPatent.

.application niet?. fipril 9, 1911i.

nu in i inn-ni"tiri i. iiiilii @n .iii iii/it.

SAME.

Peitenteol Non. 2W, llilil't. anni no. tiroteo.

bottoni outlet. B into which the discharges.

l is the new forni of agitator' which is the subject of the applicationof Paul G. Kaiser enel B. E. Reuter, filed November 20, 1913, Serial No.802,025., Steam entering the body 1 of the agitator through the pipe 21draws the contents of the tank in :it the bottom, as indicated by arro.'22, and discharges it at the top as indicated by the varrows thuscirculating the contents oi the tanli over and over again through theagitator and serving both for heating and agitation.

ther :forme of agitator may be need, but l prefer this iliorin since itproduces quicker results und is more economical to operaie is theglycerin water tank outlet 12 from the tenir A and to construct.

2 is a Steam eral pipe for admitting steam .into the space at the top ofthe tank above the mixture to prevent air from entering' the tank. 3 isa steam pipe of lead or brass provided with a perforated coil '18 forheating' the mixture by admission oiB lire sicario at the bottom. 4 isan exhaust or relief pipe for escape of surplus steam to preventexcessive pressure forming in the tank. its oud being sealed byti'ipping' into the small amount of Water contained in pan i0, so an toprevent air entering the pipe 4. 5 is a pressure gage. 6, 7 and 8 aresample cocks for drawing samples. 9 is a manhole ior ciitcring the tank.ll is a tank. tor collect ing the Water overflowing from the pan 10. l2is the outlet 7for removingthe contents ot' the tank or any partthereof. lt may :liso be uscil for charging tank n iroin the bottoni. i3is a theruionioter. if is a suit able tunnel connected with the pipe 20,which extends ilown to near the bottom oi the tank and Serves torcharging` tlic'iauk with either or all oiu the unite-riale, water,glyccrids7 acid, Saponiiier, &c. l0 is the main steam supply pipe.

Aier the contents have been raised lo the boiling by .steam from coil18, the valve in pipe .2i is cloned unil the valve 2l' opened so as toadmit Strain into the agitator, lei, il' is the well known sylplionsteam regulator. il. regulates the supply ot' steam to the agitator inaccori'lancc willi the tonipernture of the contenta ot""'ihc tankaecertained hi; the mercury pipe 17.

may produce my new article of manul'arture by' the process about to heilcecrilieil ironi the foiiowing glyeeriils Separating' n:

collectively: beet tallow, mutton tallovig', horse -fat, hog fat, butterfait, and their re spective greascsg' also whale oil, meuliaden oil,[ish oil, cocoanui oil, copra oil, peanut oil, linseed oil, cotton seedoil, palm oil, palm kernel oil, soya bean oil; also the hydrogenation orhardened products of many of these materials. particularly of corn oil,linseed oil., cotton seed oil and lish'oil.

its catalytic saponitiers l may use the uaphthalene variety of thc`class known geuerally as the Twitchell reagent, e. (j. such as isdescribed in United States Patent No. 628,503 of July ll, 1899, orPatent No. 001,003 ol March 29, 1808, or .latent No. 1,002,662 ofDecember 30, 1913, or Patent No. 1,058,633 of April 8, 1913, or PatentNo. 1,079,437 of November i013.

With the knowledge of my invention it is probable that this process maybe practised with other saponilers now or hereafter known. "i

The amount of' Catalytic saponiiier to be used in order to achieve myinvention in its best Jform may be substantially the same, but

is in general somewhat less than that which vhas been applied iucatalytic saponilication processes that do not employ my invention, suchas the well known Twitchell process. Practice has shown that in generalfrom 0.6"?, to lf/f, oi. catalytic saponifier, calculated against thequantity of fat used, is suliicient for low grades of tallow, greases,cotton or corn oil; for goed grades of fallow` cocoanut oil, or palmkernel oil, about one half of the above amount is generally sullicient.i

ln outline my present process comprises mixing a ggflycerid with about200?` of its weight of water, in which has been dissolved. or to whichhas been added say 02% of the weight of the fat oi catalytic saponicr.This mixture is suit-ably heated and agitated until approximately onethird oi' the saponiication has been accomplished. lt is then allowed tosettle out, which settling is hastened general-ly by the addition of astrong' sulfuric acid in small amount. lVhensepa ration is completethere will be found an upper white or whitish layer of fat and fattyacids, a lower layer consisting; largely of Water, and an intermediatelayer or ribbon of material. differing in color from either of the othertwo. l then withdraw the lower layer and the ribbon by suitable uwans,leavina' only they upper 'while or whiiish layer iu the apparatus. l'now add the same amount of Water and ratalylic saponilier as before andtreat until approxiinateirY another one third of saponifiration has beenaccomplishcd. l' repeat the settling and separating operation. l now ddagain 20% of Water and 0,2% of catalytic saponitier as before, completethe saponiieation, settle and separate as beior `vention by means ofthe' following' intatta In some cases it will be Afound advisable toprovide the material about to undergo saponiication Withfrec sulfuricacid to the extent of about 0.2% of the Waterin the total mix.

The progress of the saponiication is controlled in the usual manner bydetermining the acid value of the product.

l `will now proceed to illustrate my ,inu

amples, but ll Wish to be understood as 1n anywise limiting myself tothe'detaiis of proportion, operation, temperatures, or times, sincethese may be varied Within wide ranges Without in anywise departin a thespirit oit my invention: i

Pnon'ocmo FATTY ACIDS FROM Tamowi Preliminary cleansing. Pump15,000pounds oi tallow into the tank A; turn on tliesteam from pipe 8 untilboiiing ensues; agitato by agitator l; add

pounds of sulfuric acid of EBSQ@ continue boiling for one hour; turn oitthe steam and stop the agitator; settle until the i stop the agitatorand .iet settle; during this 4' settling prevent entrance of air intothe tank by causing steam to blow into the top ci the tank from thesteam seal pipe 2 througii.M out the time that the tank 1s not boiling;draw ofi' the. water and'ltiie ribbon oit-disent ered material it any,leaving the undeeonr posed fat and fatty acids in the tank.

Second Zioz'Z.

Turn on the steam in coil 18; when boiling: lis etlected start theagitator l; turn ott the steam seal pipe 2; add 3000 pounds of water, 35pounds of the catalytic saponitler; make water acid to the extent ci0.2% to 0.4% H250, by gradual addition of suliicient of the abovesulfuric acid; boil and agitato for twelve (l2) hours; proceed as underfirst boil above beyond tnis point.

T/tz'ral boil.

rrocced as under second boil by turning on the steam in coil 18, etc.;add the saine amounts of Water yand catalytic saponiier as before,determine the acidit and correct iii need be, and repeat the boiling,agitatinig latence and separating as under second boil and first boil.The material leftin the tank is the. free fatty acids; the glycerin iscontained in the Withdrawn water layers.

lVashz'ng.

Turn on the stealm in coil 18 and when boiling is effected start theagitator 1, when the seal pipe is turned ofi'. Add 1500 pounds of water,boil f or thirty minutes, then close y down as fully described underfirst boil and let settle; withdraw the lower layer and any discolored'material as under iirst, second and third boil, leaving the free fattyacids in the tank.

Neutmh'aag.

Turn on the steam in coil 18, as under Washing above, and when boilingis effected start the agitator l, when the seal pipe 2 is turned od',add barium carbonate mixed with about 150 pounds of water and boil forfifteen minutes, or until the liquid is neutral to methy1-orangeindicator; I have found 35 pounds barium carbonate usually to suffice.When neutral stop the agitator, turn ofi' all steam and let settle forone hour; draw olf all watery liquid and mix with the watery liquidsfrom the preceding iirst, second and third boils and washing. Thematerial in the ytank comprises the free fatty acids with some adher ingmoisture and these are now ready for use in making soap as given below.

While l have above describedl an equal distribution of the catalystbetween the three saponification operations, and refer that form ofprocess, I am aware t at in regulating this distribution the operatorshould have some regard to the kind and quality of stock undertreatment, but as a rule if an equal distribution is departed from Ihave found it best to have the proportions either progressively greateror progressively smaller, portion intermediate in amount between thesecond and third.

PRODUCING Soar FROM 'rmi ABOVE PRODUCT.

`Weigh 0E 2,000 pounds of the above fatty acid product; place it in asuitable tank such as a steam jacketed soa mixing machine; add thereto1000 poun s ofa caustic soda solution containing about 290 pounds ofN212() and so much more thereof as may be necessary so that the soapresulting may contain the usual small amount of free alkali; during themixing of the fatty acid and the caustic soda they should be-very wellintermingled; raise the temperature by means of steam to a temperatureranging from 170 degrees to 200 degrees F.; the progress of the actionis controlled in the usual Way'by means of the usual free alkali test.

or to have the rst pro The material thus produced is ready for furthersuitable treatment for the' production of either a colored ornon-colored soap in the usual Way.

In lieu of the above method of making the soap from the fatty acid theordinary boiling method may be employed. i

The above examples are both based upon actual factory operation, and theresults there described will be certainly obtained on repeating them inthe amounts and under the conditions described.

'In the soap making art and in the art of making fatty acids thebenefits of this invention are not realized when the amount of glyceridoperated on4 in one batch is less than' 10,000 pounds. My discovery andihvention are of such a nature that they are easily overlooked or nottaken into account in minor operations, such as laboratory andinvestigation work, and even on small factory scales,v where the unit isless than 10,000 pounds of glycerid.

y new article of manufacture may be identified by the following test,after the soap has aged for a period of ten days from the time ofproductlon. Y

I take a bar of soap which has been wrapped in the usual commercial Way,in

one or more Wrappings of paper, for at least ten days. one half and halfin the paper. I now-expose the removed half tothe action of air andsunlight, under such conditions that the soap does not come into contactwith dust or other solid material, preferably by exposing this test `barto the air and sun-light under glass in any such Way that the air hasaccess to the soap, and solid particles are excluded. At the end of thetest period, say ten days, the exposed half is compared with the wrappedhalf and will be found to be not substantially darkened in color, or mayeven be found to be lighter in color.

l have not described the introduction of any bleaching agent, and whenproperly conducted upon proper stock no bleaching agent is necessary forthe production of good results, but l do not wish to be understood aslimiting myself to the exclusion of a bleaching agent. v

By soap as used in this specification l means a soap which is a normalhard soap.

am aware that the attempt has been made to maintain the lightness ofcolor not by the treatment of the soap itself7 but by the addition tothe soap of whitening agents, such as zinc oXid or a peroxid, such assodium, zinc, calcium, hydrogen, and the like. But l do not wish to beunderstood as claiming articles in which the colori` ismaintainedsubstantiall by the admiXture of such foreign materialis.

I out the bar in half, remove securely rewrap the other Itiscommercially and economically,` prac- L30 ticable with the above processto obtain the fatty acid product substantially free from glycerin; andcommercially for soap makcontains tivo or more fatty acids.

ing I refer ,that it be substantially free from g ycerin, but I do notwish to be understoodaslimiting myself to the exclusion of glycerin.

PnonUciNe STEAM()l ACID SunSun-Nens. The fatty acid productaboveyobtained made from some of the starting glycerids,

ysuch as tallow, one or more of these fatty acids is a solid fatty acid,such as stearic acid. By separating this solid fatty acid. or stearicacid from the other constituents of tlie'fatty acid product, it may besold as such, or may be used in the manufacture of candles, ltoiletpreparations, or other articles containing soliolA fatty vacid orstearic acid, bythe same methods heretofore employed in makingsuch'artcles with ordi-4 When Which'consists in successivelyv applyingto the fats or oils under treatmentrfractional portions 'of the totalquantity 'of the saponiier employed, excluding air from contact with thematerial undergoing saponiication and removing the ribbon of impu rity,intermediate successive applications of the saponifler. v i

2. The process of producing'fatty acids With an organic catalyzer Whichconsists in successively heating the 'fatty mixture under treatment withfractional portions of the en tire quantity of the catalyzer employedfor saponifying fatty `m1Xture, excluding air from contactwith thematerials undergoing treatment, settling out the watery portion of themixture between successive beatings y v a w, thereof and removing Atheribbon of im i purity.

4 3.- As a new larticle ofk manufacture, .a solid fatty acid substancedevoid of arti'- icial coloring inateixialwliicli. after aging for aper-iod'of tendays after making, on exposure to air and sunsliglit 'fora period of ten days has its color diminished in intensity.

In testimony WliereofV I have `hereunto signed my naine in the scribingwitnesses.

BALTHASAR REUTER. Witnessesz M. E'. MCNINCH,

E. M. Locirwonny presence of tivo siib-

